Cu单原子与氧空位协同作用增强电催化CO2还原中C2液相产物活性

doi:10.1016/S1872-2067(23)64587-5

催化学报 ›› 2024, Vol. 57: 96-104.DOI: 10.1016/S1872-2067(23)64587-5

Cu单原子与氧空位协同作用增强电催化CO₂还原中C₂液相产物活性

别泉泉, 尹海波(), 王云龙, 苏海伟, 彭悦, 李俊华()

清华大学环境学院, 环境模拟与污染控制国家重点联合实验室, 北京 100084

收稿日期:2023-09-27 接受日期:2023-12-21 出版日期:2024-02-18 发布日期:2024-02-10
通讯作者: * 电子信箱: yinhaiboqifei@tsinghua.edu.cn (尹海波),lijunhua@tsinghua.edu.cn (李俊华).
基金资助:
国家自然科学基金(22206096);国家自然科学基金(21936005);博士后基金(2020TQ0166);博士后基金(2021M691771)

Electrocatalytic reduction of CO₂ with enhanced C₂ liquid products activity by the synergistic effect of Cu single atoms and oxygen vacancies

Quanquan Bie, Haibo Yin(), Yunlong Wang, Haiwei Su, Yue Peng, Junhua Li()

State Key Joint Laboratory of Environment Simulation and Pollution Control, School of Environment, Tsinghua University, Beijing 100084, China

Received:2023-09-27 Accepted:2023-12-21 Online:2024-02-18 Published:2024-02-10
Contact: * E-mail: yinhaiboqifei@tsinghua.edu.cn (H. Yin), lijunhua@tsinghua.edu.cn (J. Li).
Supported by:
National Natural Science Foundation of China(22206096);National Natural Science Foundation of China(21936005);China Postdoctoral Science Foundation(2020TQ0166);China Postdoctoral Science Foundation(2021M691771)

摘要/Abstract

摘要：

铜(Cu)因具有很好的CO结合能而被认为是目前可将CO₂电还原为乙酸、乙醇等多碳产物的重要催化材料. 虽然Cu基催化剂表现出较好的还原活性, 但产物的低选择性制约了其大规模商业化应用. 因此, 迫切需要开发高选择性、低成本的Cu基催化剂. 研究表明, 具有分散Cu-N活性位点的Cu基单原子催化剂是理想的CO₂电化学还原反应(CO₂RR)催化剂, 但仍然存在着与反应关键中间体结合能较高的难题. 当前研究多聚焦在诱导单原子的电子配位环境或催化剂的载体结构缺陷, 关于二者之间的协同作用研究较少.

本文通过简单的水热法与氢溢流策略制备了Cu单原子负载的高氧空位UIO66催化剂. X射线光电子能谱和高角度环形暗场扫描透射电子显微镜结果表明, Cu物种以高度分散的单原子形式存在. 采用X射线吸收精细结构谱和X射线光电子能谱(XPS)的N 1s能级研究了Cu原子的电子和配位结构, 证明了Cu-N键的存在. 此外, 相较于未经过H₂二次处理的Cu SAs/UIO材料和未负载Cu单原子的UIO-H₂材料, Cu SAs/UIO-H₂样品在电子顺磁光谱中观察到更加明显的氧空位信号, XPS谱的O 1s能级、傅里叶变换红外光谱(FTIR)表征结果均表明大量氧空位的存在, 从而证明成功制备了Cu单原子负载的高氧空位UIO66催化剂(Cu SAs/UIO-H₂). 反应测试结果表明, 高氧空位掺杂UIO66耦合Cu-N位点后表现较好的CO₂RR性能, 在-0.66 V (vs. RHE)的低电位下对于C₂液相产物实现了58.62%的法拉第效率, 高于大多数已报道的Cu基催化剂结果. 其中, 乙醇的法拉第效率达46.28%, 是UIO66-NH₂, Cu SAs/UIO的9.61倍和2.78倍. 经过12 h的稳定性测试后, 乙醇仍然能够维持46%的法拉第效率, 且反应后催化剂形貌和晶体结构几乎未发生改变, 表明催化剂具有较高的稳定性和实际应用前景. 为进一步分析反应机理, 利用原位FTIR技术检测*CHO, *OCCHO和*CH₃CH₂O等重要反应中间体的形成, 从而确定CO₂RR产乙醇的反应路径, 并通过密度泛函理论分析了溶剂化效应的影响, 验证了Cu单原子与大量氧空位协同作用下易于诱导关键中间体*HCCOH的生成, 提出了大量氧空位的存在降低了CO₂RR产乙醇的反应能垒的理念, 并分析计算CO₂RR产乙醇和产乙烯两条路径的能垒, 讨论Cu SAs/UIO-H₂催化剂具有高乙醇选择性的原因.

综上所述, Cu基单原子与氧空位协同是提高电催化剂CO₂RR活性的有效策略, 具有良好的应用前景. 本文为在原子尺度上设计高性能Cu单原子催化剂提供了一种新思路.

关键词: 铜单原子催化剂, 氧空位, 电催化, CO₂转换, 乙醇合成

Abstract:

Electrochemical conversion of CO₂ to high energy density multi-carbon liquid phase fuels such as ethanol offers a promising strategy to realize carbon neutrality. However, the selectivity of value-added C₂ liquid products is still deemed unsatisfactory currently due to the high overpotential, poor selectivity, and the difficulty of the C-C coupling process. Herein, we report that Cu single atoms (SAs) on hydrogen reduced UIO66-NH₂ (named Cu SAs/UIO-H₂) achieve C₂ liquid products Faraday efficiency (FE) of 58.62% and ethanol FE of 46.28% at a low potential of -0.66 V versus the reversible hydrogen electrode. The ethanol FE of Cu SAs/UIO-H₂ is 9.61 times higher than UIO66-NH₂. Moreover, the experimental results and theoretical calculations demonstrate that Cu SAs and oxygen vacancies (OVs) synergistically promote the generation of *HCCOH intermediate, thus accelerating the formation of ethanol. This work offers deeper understanding at the atomic scale for designing high-performance electrocatalysts for CO₂conversion to valuable liquid fuels.

Key words: Cu single atoms catalyst, Oxygen vacancies, Electrocatalysis, CO₂ conversion, Ethanol synthesis

别泉泉, 尹海波, 王云龙, 苏海伟, 彭悦, 李俊华. Cu单原子与氧空位协同作用增强电催化CO₂还原中C₂液相产物活性[J]. 催化学报, 2024, 57: 96-104.

Quanquan Bie, Haibo Yin, Yunlong Wang, Haiwei Su, Yue Peng, Junhua Li. Electrocatalytic reduction of CO₂ with enhanced C₂ liquid products activity by the synergistic effect of Cu single atoms and oxygen vacancies[J]. Chinese Journal of Catalysis, 2024, 57: 96-104.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(23)64587-5

https://www.cjcatal.com/CN/Y2024/V57/I2/96

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Fig. 1. (a) Synthesis process of Cu SAs/UIO-H2. Cu (green), Zr (blue), N (light blue), C (gray), O (red), H (pink). HAADF-STEM (b,c) and high-resolution HAADF-STEM (d) images of Cu SAs/UIO-H2. Cu SAs are highlighted with yellow circles. (e) TEM image and EDS mappings of Cu SAs/UIO-H2.

Fig. 2. XANES (a) and FT-EXAFS (b) spectra of Cu SAs/UIO-H2, Cu SAs/UIO, and reference samples (Cu foil, CuO and Cu2O) at Cu K-edge. WT-EXAFS spectra of CuO (c), Cu2O (d), Cu foil (e), Cu SAs/UIO (f) and Cu SAs/UIO-H2 (g). EXAFS fitting curves of Cu SAs/UIO-H2 at R-space (h) and K-space (i).

Fig. 3. (a) LSV curves of Cu SAs/UIO-H2, Cu SAs/UIO, UIO-H2 and UIO. FEs of CO2RR products of Cu SAs/UIO (b), UIO-H2 (c), and Cu SAs/UIO-H2 (d) at different potentials, respectively. (e) Comparison of FE and activities between Cu SAs/UIO-H2 and Cu-based catalysts for CO2RR to C2H5OH. (f) Stability test and the FEs of C2H5OH over Cu SAs/UIO-H2 at -0.66 V (vs. RHE) for 12 h.

Fig. 4. (a) Time-dependent in-situ DRIFTS spectra of Cu SAs/UIO-H2 for CO2RR in KHCO3 electrolyte from 2 to 90 min. (b) Calculated activation energy for CO2-to-C2H5OH and HER. (c) Schematic pathway of the CO2RR process toward ethanol synthesis. (d) Calculated free energy diagram of CO2 reduction to intermediates over the samples.

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Cu单原子与氧空位协同作用增强电催化CO₂还原中C₂液相产物活性

Electrocatalytic reduction of CO₂ with enhanced C₂ liquid products activity by the synergistic effect of Cu single atoms and oxygen vacancies

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